When GC Column Length Alone Isn’t Enough€¦ · When Length Alone Isn’t Enough •The traditional CALIDUS configuration only allows for two column modules •Falcon has now added

When GC Column Length Alone Isn’t EnoughPresented by Nate Caton of Caton Chemical Consulting, LLC.

AbstractWhen Length Alone Isn’t Enough: A Novel Two Module, Three Column Configuration (patent pending) for H2, O2, N2 and Hydrocarbons

In labs and pilot plant settings it is often necessary to have near assay-like analytics for very broad boiling range components. The selectivity necessary for fixed gas components requires sensitive column material like ShinCarbon. And to get both low boiling and higher boiling hydrocarbons requires either extreme lengths or two different column types. This paper will discuss the first commercial application of the new technology delivering very broad boiling range distribution analysis in a single Ultrafast GC.

When Length Alone Isn’t Enough

• Traditional GC’s may utilize long columns (50m+) to achieve desired separations

• This “brute force” method can be effective in certain situations, but what if there is a more powerful solution?

Traditional GC’s


• CALIDUS GC’s can use two independently temperature controlled column modules to increase selectivity

• Smaller columns (2m-16m) can be used with heartcutting to achieve the same or better separations as compared to the long columns typically seen on traditional GC’s

CALIDUS Ultrafast GC’s


• The traditional CALIDUS configuration only allows for two column modules

• Falcon has now added the ability to include a third column into a two-module configuration (patent pending) to further increase selectivityAdding a third column to the two-

module configuration

Two

independent

columns wound

on the same

ring in the

same module

How Caton Chemical Consulting Utilizes the CALIDUS

• The CALIDUS three-column GC is currently being used by Caton Chemical Consulting for testing semi-pilot plant scale experiments

• One such test includes monitoring the reactions between a feedstock containing mostly oxygen and methane as it passes through certain catalysts

• These reactions produce a variety of hydrocarbon isomers that must be separated and accurately measured

Walk-in Fume Hood Semi-Pilot Plant

Semi-Pilot Plant Left of CALIDUS on the Floor

Why Use a Three-Column Configuration?

Caton Chemical Consulting had

a problem

They needed to make fast, accurate, and precise measurements on a

variety of compounds in ppm to % ranges throughout the course of a

reaction


Separating all of the components

on one GC created the need

for a third column

Putting heavier hydrocarbon material onto the ShinCarboncolumn was not possible due to

long run times (>5 mins) and poor separation

Putting permanent gases on the Alumina Bond was not possible

due to poor/no separation


A third column, a Q-Bond, was

added to the same module as the ShinCarbon

This column helps to separate the injected components before they reach the ShinCarbon column

Properly timed column switching can then move these pre-

separated components to the appropriate column

How A Three-Column Configuration Works

A column switching valve helps to sort which compounds end up on which column after they pass through the Q-Bond

How Caton Chemical Consulting

utilizes the CALIDUS

The 4m Q-Bond serves as a sort of pre-column to separate the permanent gases from the hydrocarbons so that the heavier components are not loaded onto the ShinCarbon


Components pass from the Q-Bond onto a 2m micropackedShinCarbon column that separates permanent gases such as H2, O2, N2, CH4, CO, and CO2



The detection of the permanent gases from the ShinCarboncolumn is done using a Dielectric Barrier Discharge (DBD) detector in helium ionization mode


After activating the CS valve, a 4m Alumina Bond column separates C2-C4 hydrocarbons including several C4 isomers



Detection for the hydrocarbons eluting off of the Alumina Bond column is done using a Flame Ionization Detector (FID)

Permanent Gases Using DBD Detector(percent-levels)

1-5 % H2, O2, CO

Approx. 85 % Methane

Hydrocarbons Using FID(ppm-levels)

Hydrocarbons Using FID - Zoomed(ppm-levels)

5 ppm isobutylene

Four Overlaid DBD Chromatograms Taken Over a Period of 20 Minutes During Reaction

O2 decreasing in

concentration as reaction

continues. Methane

slightly decreasing while

all other components

increasing

Four Overlaid FID Chromatograms Taken Over a Period of 20 Minutes During Reaction

Ethane, ethylene, and

other hydrocarbons

increasing in concentration

as reaction continues

Thank You For Your Interest!

Questions??

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When GC Column Length Alone Isn’t Enough€¦ · When Length Alone Isn’t Enough •The traditional CALIDUS configuration only allows for two column modules •Falcon has now added